CN114562185A - Fluorescent composite fireproof glass and preparation method thereof - Google Patents
Fluorescent composite fireproof glass and preparation method thereof Download PDFInfo
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
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- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
- E06B3/677—Evacuating or filling the gap between the panes ; Equilibration of inside and outside pressure; Preventing condensation in the gap between the panes; Cleaning the gap between the panes
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention provides fluorescent composite fireproof glass and a preparation method thereof; the preparation method comprises the following steps: a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution; b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution; c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass. Compared with the prior art, the preparation method provided by the invention adopts specific process steps to realize better overall interaction, and the prepared fluorescent composite fireproof glass has the function of body anti-counterfeiting, and is strong in concealment, strong in ultraviolet shielding property and good in thermal stability.
Description
Technical Field
The invention relates to the technical field of luminous fireproof materials, in particular to fluorescent composite fireproof glass and a preparation method thereof.
Background
Counterfeit and inferior products are a global problem, and cause serious adverse effects on governments, industries and consumers in terms of economy and safety. Therefore, the development of reliable and safe anti-counterfeiting technology has been receiving wide attention. In the past decade, a variety of anti-counterfeiting technologies, such as plasma-based anti-counterfeiting labels, magnetic response technologies, holographic anti-counterfeiting technologies, optical anti-counterfeiting technologies, etc., have emerged. Compared with other anti-counterfeiting technologies, the cost of fluorescence anti-counterfeiting is lower, the preparation and operation are simpler, the concealment is better, and therefore the fluorescence anti-counterfeiting technology is more and more concerned. Heretofore, various luminescent materials including organic dyes, mace-based doped luminescent materials, quantum dots, and the like have been widely used in the fields of data storage and information security. However, most of optical materials used in the anti-counterfeiting field are easy to reproduce only through external fluorescent signal output, and part of luminescent materials have poor light stability and certain toxicity, so that potential safety hazards exist. Therefore, there is still a need to develop new luminescent materials with intrinsic optical signal, stable optical properties and no/low toxicity to meet the higher level anti-counterfeiting requirement.
At present, the latest generation of composite fireproof glass fireproof interlayer adopts alkaline silica sol as a raw material and carries out a curing process in a specific curing mode. The performance of the fireproof interlayer materials is different, the advantages and disadvantages of the performances such as fire resistance limit, weather resistance and the like are difficult to distinguish from the appearance, and counterfeit products are easy to appear. If a common anti-counterfeiting mode is used, the good effect is difficult to play, so a novel mode is needed to provide anti-counterfeiting capability for the composite fireproof glass.
Disclosure of Invention
In view of the above, the present invention provides a fluorescent composite fireproof glass and a preparation method thereof, the nitrogen-hybridized blue light carbon-based molecular solution prepared by the present invention is prepared simply and efficiently by a hydrothermal method, and is doped into the composite fireproof glass, such that the composite fireproof glass is provided with a specific anti-counterfeiting function, and the ultraviolet isolation property and the thermal stability of the composite fireproof glass are enhanced.
The invention provides a preparation method of fluorescent composite fireproof glass, which comprises the following steps:
a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution;
b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution;
c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass.
Preferably, the carbon-based precursor in step a) is selected from one or more of citric acid, ammonium citrate and phloroglucinol; the nitrogen-containing substance is selected from one or more of ethanolamine, o-phenylenediamine and urea; the silane coupling agent is selected from gamma-aminopropyltriethoxysilane and/or 3- (2-aminoethylamino) propyltrimethoxysilane.
Preferably, the mass ratio of the carbon-based precursor, the nitrogen-containing substance, the silane coupling agent and the water in the step a) is 1: (0.1-2): (0.5-1): (25-100).
Preferably, the temperature of the hydrothermal reaction in the step a) is 170-200 ℃ and the time is 1-3 h.
Preferably, the concentration of the alkaline silica sol in step b) is 40 to 60 wt%; the concentration of the potassium hydroxide aqueous solution is 40 wt% -60 wt%.
Preferably, the mass ratio of the alkaline silica sol, the glycerol, the nitrogen-hybridized blue light carbon-based molecular solution and the potassium hydroxide aqueous solution in the step b) is (100-120): (10-15): (1-3): (40-50).
Preferably, the reaction temperature in the step b) is 40-55 ℃, and the reaction time is 20-40 min.
Preferably, the stirring time in step b) is 5min to 15 min.
Preferably, the curing temperature in the step c) is 75-85 ℃ and the curing time is 5-8 h.
The invention also provides fluorescent composite fireproof glass prepared by the preparation method of the technical scheme.
The invention provides fluorescent composite fireproof glass and a preparation method thereof; the preparation method comprises the following steps: a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution; b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution; c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass. Compared with the prior art, the preparation method provided by the invention adopts specific process steps to realize better integral interaction, wherein the preparation method of the nitrogen-hybridized blue light carbon-based molecular solution is simple, the cost of synthetic raw materials is low, the product does not need to be purified, and the preparation method is green, pollution-free, low in toxicity and suitable for batch production; the prepared fluorescent composite fireproof glass has the function of body anti-counterfeiting, and is strong in concealment, strong in ultraviolet shielding property and good in thermal stability.
Meanwhile, the preparation method provided by the invention has the advantages of simple process, low energy consumption, economy, environmental protection and the like, and the cost of the synthetic raw materials is low, so that the preparation method has good application prospect and potential in the technical field of luminous fireproof materials.
Drawings
FIG. 1 is a transmittance curve of nitrogen-hybridized blue-light carbon-based molecular solution prepared in example 1 at different wavelengths;
FIG. 2 is a photograph of the nitrogen-hybridized blue-light carbon-based molecular solution prepared in example 1 before and after irradiation with 365nm light;
FIG. 3 is a graph of the emission spectrum of the nitrogen-hybridized blue-light carbon-based molecular solution prepared in example 1 under the irradiation of light with a wavelength of 365nm under neutral and alkaline conditions;
FIG. 4 is a graph of the emission spectra of the nitrogen-hybridized blue-light carbon-based molecular solution prepared in example 1 under different excitations;
FIG. 5 is a graph showing the emission spectra of the composite fire-resistant glass prepared in example 1 and comparative example 1 under 365nm excitation;
FIG. 6 is a DTG curve for the composite fire resistant glass interlayers prepared in example 1 and comparative example 1;
FIG. 7 is a transmittance curve of the composite fire resistant glass prepared in example 1 and comparative example 1 at different wavelengths;
FIG. 8 is a temperature rise curve of the back fire surface of the composite fire-proof glass prepared in example 1 and comparative example 1;
FIG. 9 is a photograph of the composite fire-resistant glass prepared in example 1 and comparative example 1 before and after irradiation with 365nm light.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of fluorescent composite fireproof glass, which comprises the following steps:
a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution;
b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution;
c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass.
According to the preparation method, a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water are mixed, then hydrothermal reaction is carried out, and nitrogen-hybridized blue light carbon-based molecular solution is obtained after cooling.
In the present invention, the carbon-based precursor is preferably selected from one or more of citric acid, ammonium citrate and phloroglucinol, more preferably citric acid, ammonium citrate or phloroglucinol; the nitrogen-containing substance is preferably selected from one or more of ethanolamine, o-phenylenediamine and urea, more preferably ethanolamine, o-phenylenediamine or urea; the silane coupling agent is preferably selected from gamma-aminopropyltriethoxysilane and/or 3- (2-aminoethylamino) propyltrimethoxysilane, more preferably gamma-aminopropyltriethoxysilane or 3- (2-aminoethylamino) propyltrimethoxysilane. The sources of the carbon-based precursor, the nitrogen-containing substance, and the silane coupling agent are not particularly limited, and commercially available products known to those skilled in the art may be used.
In the present invention, the mass ratio of the carbon-based precursor, the nitrogen-containing substance, the silane coupling agent, and water is preferably 1: (0.1-2): (0.5-1): (25-100), more preferably 1: (0.5-1.2): (0.5-1): (62.5 to 100).
The mixing method is not particularly limited in the present invention, and ultrasonic agitation well known to those skilled in the art is employed to uniformly mix the raw materials.
In the invention, the hydrothermal reaction process is preferably carried out in a hydrothermal kettle; the temperature of the hydrothermal reaction is preferably 170-200 ℃, more preferably 170-180 ℃, and the time is preferably 1-3 h; and after the hydrothermal reaction is completed, naturally cooling to obtain the nitrogen-hybridized blue light carbon-based molecular solution.
After the nitrogen-hybridized blue light carbon-based molecular solution is obtained, alkaline silica sol and glycerol are mixed, water with the same mass as that of the glycerol is removed through concentration, the obtained nitrogen-hybridized blue light carbon-based molecular solution and a potassium hydroxide aqueous solution are sequentially added to react, and then the mixture is stirred and cooled under the vacuum condition to obtain groutable intermediate liquid.
In the present invention, the concentration of the alkaline silica sol is preferably 40 to 60 wt%, more preferably 50 wt%; the concentration of the aqueous potassium hydroxide solution is preferably 40 to 60 wt%, more preferably 50 wt%. The source of the alkaline silica sol and the aqueous solution of potassium hydroxide is not particularly limited in the present invention, and commercially available products or self-products known to those skilled in the art may be used.
In the invention, the mass ratio of the alkaline silica sol, the glycerol, the nitrogen-doped blue light carbon-based molecular solution and the potassium hydroxide aqueous solution is preferably (100-120): (10-15): (1-3): (40-50), more preferably 100: 10: 1.5: 40.
in the present invention, the reaction temperature is preferably 40 to 55 ℃, more preferably 50 ℃, and the reaction time is preferably 20 to 40min, more preferably 30 min. In the invention, the obtained nitrogen-hybridized blue light carbon-based molecular solution and a potassium hydroxide aqueous solution are sequentially added for reaction, preferably, after the nitrogen-hybridized blue light carbon-based molecular solution is added, the mixed solution is heated to the temperature of the reaction, and then the potassium hydroxide aqueous solution is added for constant-temperature reaction.
In the present invention, the stirring time is preferably 5 to 15min, and more preferably 10 min.
After the groutable intermediate liquid is obtained, the groutable intermediate liquid is injected into a cavity between the glass interlayers, and the fluorescent composite fireproof glass is obtained after curing.
In the present invention, the curing temperature is preferably 75 to 85 ℃, more preferably 80 ℃, and the time is preferably 5 to 8 hours, more preferably 7 hours.
The preparation method provided by the invention comprises the steps of carrying out in-situ synthesis on a nitrogen-hybridized blue-light carbon-based molecular solution by using a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water according to a specific ratio through a one-step hydrothermal method, and preparing the fluorescent composite fireproof glass by using 100-120 parts by weight of alkaline silica sol, 10-15 parts by weight of glycerol, 40-50 parts by weight of potassium hydroxide solution and 1-3 parts by weight of nitrogen-hybridized blue-light carbon-based molecular solution as components; the preparation method of the aza blue light carbon-based molecular solution is simple, the cost of synthetic raw materials is low, the product does not need to be purified, and the aza blue light carbon-based molecular solution is green, pollution-free, low in toxicity and suitable for batch production; the composite fireproof glass provided by the invention has the advantages that the anti-counterfeiting function of the body is provided for the composite fireproof glass, the concealment is strong, and the ultraviolet shielding property and the thermal stability are enhanced.
The invention also provides fluorescent composite fireproof glass prepared by the preparation method of the technical scheme.
The invention has the following beneficial effects:
the nitrogen-hybridized blue light carbon-based molecular solution provided by the invention has the function of absorbing ultraviolet light (300-400 nm), is low in preparation cost, simple and rapid in preparation method, only needs hydrothermal reaction, does not need purification and separation, and is environment-friendly; and the fluorescent material has the characteristics of no fluorescence quenching under alkaline conditions, easy combination with silica sol, colorless and transparent aqueous solution and the like. When the composite fireproof glass is doped into fireproof inorganic hydrogel, the light transmittance and the color cannot be influenced at first, the ultraviolet light absorption capacity of the composite fireproof glass is enhanced, the damage of sunlight to a human body is reduced, the light transmission of other wavelengths is not influenced, and the thermal stability of an interlayer can be improved finally.
The invention fills the blank of the anti-counterfeiting mode of the composite fireproof glass body, and the prior art does not have a material which can not only realize the specific anti-counterfeiting of the body, but also can not generate negative influence on the sandwich material of the composite fireproof glass.
The invention provides fluorescent composite fireproof glass and a preparation method thereof; the preparation method comprises the following steps: a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution; b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution; c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass. Compared with the prior art, the preparation method provided by the invention adopts specific process steps to realize better overall interaction, wherein the preparation method of the nitrogen-hybridized blue-light carbon-based molecular solution is simple, the cost of synthetic raw materials is low, the product does not need to be purified, and the preparation method is green, pollution-free, low in toxicity and suitable for batch production; the prepared fluorescent composite fireproof glass has the function of body anti-counterfeiting, and is strong in concealment, strong in ultraviolet shielding property and good in thermal stability.
Meanwhile, the preparation method provided by the invention has the advantages of simple process, low energy consumption, economy, environmental protection and the like, and the cost of the synthetic raw materials is low, so that the preparation method has good application prospect and potential in the technical field of luminous fireproof materials.
To further illustrate the present invention, the following examples are provided for illustration. The starting materials used in the following examples of the present invention are all commercially available.
Example 1
S1, weighing 0.4 part by weight of ammonium citrate, 0.2 part by weight of urea, 0.2 part by weight of gamma-aminopropyltriethoxysilane and 25 parts by weight of water, mixing in a beaker, ultrasonically stirring to completely mix the substances, transferring to a hydrothermal kettle, carrying out hydrothermal reaction at 170 ℃ for 1h, and naturally cooling to obtain an aza blue light carbon-based molecular solution;
s2, weighing 100 parts by weight of 50 wt% alkaline silica sol and 10 parts by weight of glycerol, uniformly mixing, concentrating to remove 10 parts by weight of water, uniformly mixing with 1.5 parts by weight of the nitrogen-doped blue light carbon-based molecular solution obtained in the step S1, adding 40 parts by weight of 50 wt% potassium hydroxide aqueous solution, mixing and reacting at 50 ℃ for 30min, vacuumizing the system, stirring for 10min under a vacuum condition, and cooling to obtain groutable intermediate solution;
and S3, injecting the groutable intermediate liquid obtained in the step S2 into a cavity between the glass interlayers, and curing at 80 ℃ for 7 hours to obtain the fluorescent composite fireproof glass.
Example 2
The preparation method provided by the embodiment 1 is adopted to obtain the fluorescent composite fireproof glass; the differences are that:
s1, weighing 0.4 part by weight of citric acid, 0.3 part by weight of ethanolamine, 0.3 part by weight of gamma-aminopropyltriethoxysilane and 25 parts by weight of water, mixing in a beaker, carrying out ultrasonic stirring to completely mix the substances, transferring to a hydrothermal kettle, carrying out hydrothermal reaction at 170 ℃ for 2 hours, and naturally cooling to obtain the nitrogen-hybridized blue-light carbon-based molecular solution.
Example 3
The preparation method provided by the embodiment 1 is adopted to obtain the fluorescent composite fireproof glass; the difference lies in that:
s1, weighing 0.25 part by weight of phloroglucinol, 0.3 part by weight of o-phenylenediamine, 0.25 part by weight of 3- (2-aminoethylamino) propyl trimethoxy silane and 25 parts by weight of water, mixing the materials in a beaker, carrying out ultrasonic stirring to completely mix the materials, transferring the mixture to a hydrothermal kettle, carrying out hydrothermal reaction at 180 ℃ for 3 hours, and naturally cooling to obtain the nitrogen-hybridized blue-light carbon-based molecular solution.
Comparative example 1
S1, weighing 100 parts by weight of 50 wt% alkaline silica sol and 10 parts by weight of glycerol, uniformly mixing, concentrating to remove 10 parts by weight of water, adding 40 parts by weight of 50 wt% potassium hydroxide aqueous solution, mixing and reacting at 50 ℃ for 30min, vacuumizing the system, stirring for 10min under a vacuum condition, and cooling to obtain a groutable intermediate solution;
s2, injecting the grouting intermediate liquid obtained in the step S1 into a cavity between the glass interlayers, and curing for 7 hours at 80 ℃ to obtain the composite fireproof glass.
Carrying out various performance tests on the fluorescent composite fireproof glass obtained in the examples 1-3 and the composite fireproof glass obtained in the comparative example 1; obtaining the light transmittance of each fireproof glass through a light transmittance test; performing hardness test on the fireproof gel by using a Shore durometer; the apparent mass of each fire-resistant glass was observed by naked eyes.
The test results are shown in table 1.
TABLE 1 data of various properties of the fluorescent fire-resistant glass compositions obtained in examples 1 to 3 and the fire-resistant glass composition obtained in comparative example 1
| Examples | Transmittance (a) | Shore hardness/HD | Apparent mass | Limit of fire resistance |
| Example 1 | 85.5 | 96 | Colorless and colorless | ≥90min |
| Example 2 | 85.4 | 96 | Colorless and colorless | ≥90min |
| Example 3 | 85.4 | 95 | Colorless and colorless | ≥90min |
| Comparative example 1 | 85.6 | 96 | Colorless and colorless | ≥90min |
The test results in table 1 show that the fluorescent composite fireproof glass obtained in embodiments 1 to 3 of the present invention has a transmittance of more than 85%, a shore hardness of more than 95HD, and a colorless apparent mass, and it is proved that the nitrogen-doped blue light carbon-based molecular solution provided by the present invention does not have any negative effect on the performance of the composite fireproof glass.
Fig. 1 shows that the solution of aza-blue carbon-based molecule of example 1 shows a significant transmittance decrease at 339nm, and a large amount of absorption of light at this wavelength, which is the result of n → pi transition of C ═ O, and the transmittance under visible light is close to 100%, indicating that it has colorless and transparent properties. FIG. 2 shows the phenomenon that the solution of nitrogen-hybridized blue-light carbon-based molecule in example 1 is colorless and transparent under sunlight and emits blue light under 365nm excitation. Fig. 3 shows that the aza-blue carbon-based molecular solution in example 1 emits stronger light under 365nm light excitation, and the emission intensity of 365nm irradiation does not change at all under neutral and alkaline conditions, which proves that strong base does not change or destroy the luminescence center and structure of the aza-blue carbon-based molecular solution. As can be seen from fig. 4, the fluorescence spectrum of the aza-blue carbon-based molecular solution in example 1 is very pure, and has a single fluorescence peak at 440nm, the full half-peak width is about 70nm, the fluorescence is typically non-excitation wavelength-dependent, and the emission peak under the excitation of light of 250nm to 390nm is always kept at 440nm, which is consistent with the light emission inference of n → pi transition of C ═ O, and is an ideal fluorescent anti-counterfeiting material.
Fig. 5 shows that the composite fire-resistant glass of example 1 and comparative example 1 shows completely different emission spectra under 365nm excitation, comparative example 1 does not emit light with any wavelength under 365nm excitation, and example 1 emits blue light around 450 nm. Meanwhile, the composite fireproof glass interlayers of the embodiment 1 and the comparative example 1 are subjected to a thermal stability test, and as can be seen from fig. 6, the composite fireproof glass interlayer prepared in the embodiment 1 is subjected to a right shift in a 200-300 ℃ combined water absorption peak, which proves that the nitrogen-hybridized blue light carbon-based molecular solution provided by the invention enhances the thermal stability of the composite fireproof glass interlayer. Fig. 7 shows that the transmittance of the composite fire-resistant glass prepared in example 1 in the ultraviolet region is lower than that of comparative example 1, which proves that the capability of blocking ultraviolet light is enhanced, and the curves in the visible region are basically overlapped, which proves that example 1 and comparative example 1 still maintain colorless and transparent appearance. Fig. 8 shows that the fire resistance of the composite fire-proof glass added with the blue-light carbon-based molecular solution is improved before 40min, which corresponds to fig. 6, and the final fire resistance limit of the composite fire-proof glass is not negatively influenced. Fig. 9 shows that two kinds of composite fireproof glass can be effectively distinguished under 365nm irradiation, and the anti-counterfeiting effect of the body is achieved.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of fluorescent composite fireproof glass comprises the following steps:
a) mixing a carbon-based precursor, a nitrogen-containing substance, a silane coupling agent and water, carrying out hydrothermal reaction, and cooling to obtain an aza blue light carbon-based molecular solution;
b) mixing alkaline silica sol and glycerol, concentrating to remove water with the same mass as the glycerol, sequentially adding the nitrogen-hybridized blue light carbon-based molecular solution obtained in the step a) and a potassium hydroxide aqueous solution for reaction, and then stirring and cooling under a vacuum condition to obtain a groutable intermediate solution;
c) injecting the groutable intermediate liquid obtained in the step b) into the cavity between the glass interlayers, and curing to obtain the fluorescent composite fireproof glass.
2. The method according to claim 1, wherein the carbon-based precursor in step a) is selected from one or more of citric acid, ammonium citrate and phloroglucinol; the nitrogen-containing substance is selected from one or more of ethanolamine, o-phenylenediamine and urea; the silane coupling agent is selected from gamma-aminopropyltriethoxysilane and/or 3- (2-aminoethylamino) propyltrimethoxysilane.
3. The method according to claim 1, wherein the mass ratio of the carbon-based precursor, the nitrogen-containing substance, the silane coupling agent, and the water in step a) is 1: (0.1-2): (0.5-1): (25-100).
4. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction in step a) is 170 ℃ to 200 ℃ and the time is 1h to 3 h.
5. The method according to claim 1, wherein the concentration of the alkaline silica sol in step b) is 40-60 wt%; the concentration of the potassium hydroxide aqueous solution is 40 wt% -60 wt%.
6. The preparation method of claim 1, wherein the mass ratio of the alkaline silica sol, the glycerol, the nitrogen-hybridized blue-light carbon-based molecular solution and the potassium hydroxide aqueous solution in the step b) is (100-120): (10-15): (1-3): (40-50).
7. The method according to claim 1, wherein the reaction temperature in step b) is 40 to 55 ℃ and the reaction time is 20 to 40 min.
8. The method according to claim 1, wherein the stirring time in step b) is 5 to 15 min.
9. The method according to claim 1, wherein the curing in step c) is carried out at a temperature of 75 ℃ to 85 ℃ for 5h to 8 h.
10. A fluorescent composite fireproof glass, which is characterized by being prepared by the preparation method of any one of claims 1 to 9.
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| JP2021080346A (en) * | 2019-11-18 | 2021-05-27 | 冨士色素株式会社 | Phosphor composition and manufacturing method thereof |
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| CN206091064U (en) * | 2016-08-15 | 2017-04-12 | 王振鹏 | Glass system of multi -functional air purification function |
| CN111164991A (en) * | 2017-10-04 | 2020-05-15 | Ａｇｃ株式会社 | Glass plate structure and vibration plate |
| CN110627383A (en) * | 2019-10-30 | 2019-12-31 | 应急管理部天津消防研究所 | Preparation method of transparent fireproof gel and composite fireproof glass |
| JP2021080346A (en) * | 2019-11-18 | 2021-05-27 | 冨士色素株式会社 | Phosphor composition and manufacturing method thereof |
| CN112226231A (en) * | 2020-10-20 | 2021-01-15 | 重庆邮电大学 | Multicolor fluorescent carbon quantum dot and preparation method and application thereof |
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